Ultrasound techniques can be categorized into two distinct types: acoustic emission (passive mode) and ultrasound spectroscopy (active mode). Both of these techniques have many applications.

The technique of acoustic emission is based on the detection and analysis of sound produced by a process or system. This is essentially equivalent to listening to the process or system, although these sounds are often well above the frequencies that can be detected by the human ear. Generally, frequencies up to about 15 kHz are audible.

In the case of ultrasound spectroscopy, the instrument is designed to generate ultrasound waves across a defined frequency range. These waves travel through the sample and are measured using a receiver. An analogy can be drawn with UV-visible or IR spectroscopy in that the detected ultrasound spectrum reflects changes in velocity or sound attenuation due to the interaction with a sample across a range of frequencies. However, as the scope of this chapter is limited to acoustic emission, ultrasound spectroscopy will not be discussed further.

Acoustic emission is well-known in the study of fracture mechanics and therefore is used extensively by material scientists. It is also widely used as a nondestructive testing technique and is applied routinely for the inspection of aircraft wings, pressure vessels, load-bearing structures, and components. Acoustic emission is also used in the engineering industry for the monitoring of machine tool wear.

In terms of pharmaceutical applications, the dependence of the acoustic emission measurement on physical properties such as particle size, mechanical strength, and cohesivity of solid materials allows the technique to be used for the control and endpoint detection of processes such as high shear granulation, fluid bed drying, milling, and micronization.

General Principles

Acoustic emissions can propagate by a number of modes. In solids, compressional and shear or transverse modes are important. Compressional modes have the highest velocity and thus reach the acoustic detector (or acoustic emission transducer) first. However, in most process applications of acoustic emission, there are many sourceseach producing short bursts of energyand, consequently, the different modes cannot easily be resolved. The detected signal, for example on the wall of a vessel, is a complex mixture of many overlapping waveforms resulting from many sources and many propagation modes.

At interfaces, depending on the relative acoustic impedance of the two materials, much of the energy is reflected back towards the source. In a fluidized bed, for example, acoustic emissions will only be detected from particles directly impacting the walls of the bed close to the transducer.

A convenient method of studying acoustic emission from processes is to use the average signal level. A root mean square-to-direct current (RMS-to-DC) converter may be used to convert the amplitude-modulated (AM) carrier into a more slowly varying DC signal. This is referred to as the average signal level (ASL). The ASL can then be digitally sampled (typically at a sampling frequency of about 50 Hz) and stored electronically for further signal processing.

The simplest way of studying the acoustic data is to examine changes in the ASL. However, other information can be derived from examining the power spectrum of the ASL. The power spectrum is calculated by taking the complex square of the amplitude spectrum and can be obtained by performing a Fast Fourier Transform (FFT) on the digitized raw data record. Power spectra may be averaged to produce a reliable estimate of power spectral density or to give a fingerprint of a particular process regime. Interpretation of the power spectrum is complicated by the fact that the acoustic signal originating in the system is distorted by several factors including transmission, reflection, and signal transfer characteristics.

The shape of the power spectrum of the ASL record is a function of the process dynamics. Periodic processes (e.g., mechanical stirring or periodic bubbling of a fluidized bed) show high power at certain discrete frequencies. Random processes show either flicker type properties, where power is inversely proportional to frequency, or white noise type properties in which power is independent of frequency. The amplitude of the power spectrum is also affected by the energy of the acoustic emissions produced by the process. For example, if hard material is being processed, the acoustic emission produced by particle impact will be greater than that produced by soft material.

INSTRUMENTATION

Generally, piezoelectric sensors are used to detect and quantify the acoustic signals produced by a process. Piezoelectric transducers are constructed from piezoelectric crystalline solids connected to transducer control circuitry by electrical leads. When configured as a detector, an acoustic wave that impinges on the piezoelectric element is transformed into an electrical signal in the transducer control circuitry. When configured as an acoustic generator, an electrical signal applied to the piezoelectric element by the control circuitry creates an acoustic wave that can propagate into the medium to which the transducer is attached. Typically, this means that acoustic emission detectors can also be operated as acoustic wave generators and this feature is used to ensure good sensor performance as described later (see Qualification and Verification of Acoustic Emission Instruments).

In general acoustic emission applications, sensors with different resonance frequencies are often used (e.g., 70 and 190 kHz, although higher frequencies may be more appropriate at smaller scales of operation), incorporating various band-passes. As sound (ultrasound) of the appropriate frequency range reaches these sensors, an electrical signal is generated, the amplitude of which is directly proportional to the energy (amplitude) of the incident sound waves.

These signals are processed through the following:

a pre-amplifier (which incorporates signal filtering),

an RMS-to-DC converter,

a variable gain amplifier, and

a PC-based data acquisition board.

The controlling software is also incorporated into the PC.

Acoustic emission equipment generally allows several sensors to be used simultaneously by incorporating multiple electronic channels into a single instrument.

Signal Processing

The signal from a resonant transducer resembles an AM radio signal. At the resonance frequency of the transducer, the signal consists of a carrier wave that is modulated in amplitude by the process. An RMS-to-DC converter is used to demodulate the signal. The output of this device is the modulation signal or envelope.

The envelope is digitally resampled at a frequency appropriate for the process. For example, 50 Hz is a typical digital sampling rate for a fluid bed drier or high shear granulator.

FACTORS AFFECTING MEASUREMENT

The following factors can affect the acoustic data obtained and should be considered when installing an acoustic emission system.

Failure or Physical DamageAs with any other type of sensor, acoustic emission sensors can fail with time or as a result of physical damage. It is important to check the sensor function as part of routine maintenance of the instrument. If multiple sensors are installed on the same vessel, an active signal can be generated from one sensor and this can be used to check the detection on another sensor. This exercise would ensure that the sensors are detecting the acoustic signals generated by the process. A statistically valid minimum acceptable acoustic signal for the sensor(s) should also be determined and monitored at the start, middle, and end of a process to ensure the performance of the sensor(s) during a process run. This may be established from the routine maintenance signal experiments or on the basis of historical data for the sensors.

Issues of Sensor InterfacingSensors are typically installed on the outer wall of the process vessel. Several types of adhesives (temporary or permanent) can be used to attach the sensor to the vessel wall. Through repeated cleaning and vessel movement, it is possible for the bonding between the sensor and vessel to be compromised. Checking the integrity of the installation should be part of routine maintenance. Similar to item 1 above, an active signal can be used to ensure proper bonding between sensor and vessel and helps to confirm the matching of acoustic impedance.

Influence of Mechanical NoiseThe use of high frequencies significantly reduces the contribution of mechanical noise to the acoustic signal detected, especially at smaller scales of operation, although it does not eliminate it completely. Testing the effect of various motor settings, for example, can determine if the acoustic signal detected is a function of mechanical noise. If the effect is significant, using higher frequencies may be necessary. Awareness of the contribution of the mechanical noise, no matter how small, is important to consider as the motors age or are replaced.

Influence of Vessel Wall CharacteristicsBecause the sensors are often placed on the outer vessel wall, wall thickness can affect the quality of the signal detected. If the vessel is jacketed, the amplitude of the acoustic signal may be reduced. Adding more sensors on the vessel can improve signal quality. Alternatively, an increase in signal may be obtained by positioning sensor(s) at a location where contact exists between the inner and outer walls, essentially providing a waveguide between the sensor and sound source. Waveguides may also be incorporated into the design of manufacturing equipment to enable utilization of acoustic emission monitoring. Appropriate validation is required to ensure that this does not adversely affect the performance of equipment.

Effect of Material PropertiesDuring operation, the acoustic signal collected is a summation of various events occurring within the process. For example, the acoustic signal generated as particles hit the wall in a granulator is a function of the material properties of the granules (i.e., density, size, porosity). Therefore, significant changes to any of these parameters can affect the acoustic signal and the quality of the ensuing prediction.

Influence of Process-Related FactorsSimilar to item 5 above, the process-related properties (i.e., force of impact, frequency of impact, amount of material) can also affect the acoustic signal and the quality of the ensuing prediction.

Impact of Environmental ConditionsFinally, the influence of environmental factors (i.e., temperature, humidity) must also be considered.

The acoustic emission data collected is vessel/equipment specific. It is not advisable to apply a model generated on one piece of equipment to another because the acoustic information can differ as a result of the issues discussed in items 3, 4, and 5 above.

Qualification and Verification of Acoustic Emission Instruments

A system suitability approach should be taken around instrument performance, establishing optimum measurement configuration, then comparing the instrument performance to the values obtained during routine use to those obtained during installation qualification (IQ).

This approach effectively answers the issues related to sampling because, unlike other on-line analytical systems, the transducers can be optimally positioned and attached to receive the maximum signal without vessel modification.

Sample rates need to comply with the Nyquist sampling theorem, which states that a signal must be sampled at a rate that is twice the highest frequency component in the signal. A low-pass filter should be used to remove the frequency components greater than half the sampling frequency (Nyquist frequency). Failure to comply with this criterion will result in aliasing.

Owing to the nature of the piezoelectric transducers and because resonance frequencies are natural properties of the crystals, it is not necessary to test the variation (reproducibility) or drift in the frequency domain. If other types of transducers are used, this may be necessary. Any gross change in the frequency domain will be recorded as a drop in the power intensity at the resonance frequency, and therefore is covered by the power intensity tests.

The two main areas for instrument performance verification are power intensity and timings. Any change in the signal intensity will affect the raw signal and the ASL and, therefore, will also affect the power spectrum. Changes in power intensity can occur as a result of changes in the process (e.g., variation in hardness or moisture in the particles impacting the vessel wall) or changes in the acoustic conduit from the process to transducer.

Reproducibility of the acoustic conduit should be tested using a second transducer to input a pulse or ping at the resonance frequency of the receiving sensor. This reproducibility value represents the noise of the signal and can be used in calculations of limit of detection (LOD) and limit of quantitation (LOQ), where LOD is defined as three times the noise of the signal and LOQ is ten times the noise of the signal. The noise on the background signal level (in acoustic emission this background signal is mainly due to amplifier noise) should be calculated from twenty sequential ASL values acquired at the sampling frequency used for normal operation. This test should be repeated in reverse in order to establish that statistically similar intensity values can be obtained on both channels.

Short term reproducibility allows the calculation of noise. However, it does not give a measure of integrity of acoustic conduit over time or, more specifically, of changes caused by the process (e.g., variations in adhesive properties with process changes such as heating/cooling). The noise test should be repeated while executing the normal processing parameters (using an empty vessel) and the drift in the ASL should be calculated. Care should be taken to make sure that signal drift (due to normal variation in processing parameters) does not impact chemometric models used for endpoint determination. For trend plots, it should be shown that drift is not statistically significant; otherwise, drift correction will need to be applied. Values for noise, drift, and absolute ASL should be recorded and logged, and the tests re-executed if changes are made to the processing equipment or to the acoustic emission system. If no changes are made, then the tests should be re-executed every month. In this way the quality of the acoustic conduit can be shown to be intact and any changes to the signal intensity isolated and attributed to the process itself.

During routine use, it is recommended that the noise test be executed (as above) before each process run, and that power intensity and noise be calculated. These values should be logged and compared to those generated both during previous use and during installation. Impact of the deviation from previous values will be a function of the prediction model and should be addressed by method validation.

The noise data (from above) can also be used to calculate the time of flight of the pulse. If the pulse activation and signal reception are synchronized, the time taken for the pulse to transmit across the vessel can be measured. This is a good indication of the measurement electronics as well as the overall condition of the acoustic conduit. However, this test should be regarded as a measure of the system condition and needs to be executed only if changes have been made to the process equipment or the acoustic emission system, or every 6 months. Correlation of the measured timings with the historical ones should be statistically valid. If not, it is an indicator that the acoustic emission system may need requalification by the instrument manufacturer or supplier, or that there are changes in the acoustic conduit.

All of these tests require the use of an acoustic pulse generated electrically. Failure in any of the above tests could be attributed to the signal generation itself. It is recommended that the electrical pulse generation system be requalified and certified against National Institute of Standards and Technology (NIST) traceable standards every 12 months.

DATA ANALYSIS

Acoustic emission from granulators and fluid bed driers is known as continuous acoustic emission. Continuous acoustic emission is aphasic (i.e., there are no starts or stops to the signal). This means that it is unnecessary to use signal processing techniques that preserve phase. Power spectral analysis is a useful technique in processing acoustic emission signals. The information in the power spectra, unlike the raw acoustic emission signals, is coherent in the short term, allowing signal averaging to be performed. This provides a better estimate of power spectral density than that provided by a single power spectrum.

To detect endpoints in batch processes (e.g., granulation or drying endpoint), a qualitative multivariate model is appropriate (e.g., PCA or SIMCA). The following sequence of operations is performed:

Training/CalibrationAcoustic emission spectra that are representative of the endpoint condition are obtained.

ModelingA multivariate model describing the distribution of acoustic emission signals at the endpoint condition is created.

PredictionAcoustic emission spectra are compared against the model. The fit to the model (usually expressed in terms of a number of standard deviations) is monitored. As the system approaches the endpoint, the fit improves and completion of the process is established once the model fits predefined criteria. The prediction model is generated from acoustic emission spectra obtained from the process operating under normal conditions. Upsets (e.g., unwanted agglomeration in coaters) are detected by observing statistically valid deviations from the model.

Adaptive modeling has also been proposed for upset detection. This involves generating multivariate models continuously as the acoustic emission signals are acquired. Unusual deviation of the acoustic emission signal indicates the occurrence of a process upset. The advantage of adaptive modeling is that it is not necessary to perform a separate calibration step.

GLOSSARY

Acoustic Emission TransducerA solid state device usually incorporating a piezoelectric element to convert the acoustic emission wave to an electrical signal.

Acoustic ImpedanceAcoustic impedance (Z) is defined as Z = v (where is density and v is the sound velocity). It is an important quantity and gives the proportion of sound energy transmitted from one medium to another and the amount of energy reflected at the interface.

Adaptive ModelingA method that predicts the state of a process without the use of a previously generated model (i.e., there is no prior training or calibration step).

AliasingSpurious low frequency components, appearing in the signal, that are really frequencies above the Nyquist frequency.

AmplitudeThe magnitude or strength of a varying waveform.

Average Signal Level (ASL)A measure of the average power in an acoustic emission signal.

Continuous Acoustic EmissionAcoustic emission signals that cannot be separated in time and are typical of pharmaceutical processes such as granulation and fluid bed drying.

Flicker Type PropertiesA type of signal associated with many natural processes. The characteristics of flicker noise are that the power of the noise is directly proportional to the signal and has approximately a 1/f (f = frequency) spectral density distribution.

GainThe amplification factor for a component usually expressed in terms of decibels (dB).

Gain in dB = 20 log10 (Voltageout Voltagein).

Nyquist FrequencyThe Nyquist frequency is defined as half the digital sampling rate and is the highest frequency that can be reproduced faithfully.

PiezoelectricA material which generates an electric field when compressed. Piezoelectric materials are used in the construction of acoustic emission sensors. A common material is PZT (lead zirconium titanate).

Power SpectrumA power spectrum of a signal is a representation of the signal power as a function of frequency. A power spectrum is calculated from the time domain signal by means of the Fast Fourier Transform (FFT) algorithm. It is useful to study acoustic emission signals in the frequency or spectral domain, as the spectrum is often characteristic of the mechanism. Improvements in signal-to-noise ratio can be obtained by averaging a number of power spectra, as they are coherent.

Power Spectral DensityThe measure of acoustic emission power in each resolution element of the power spectrum.

Resonance FrequencyThe frequency at which an acoustic emission sensor is most sensitive. Resonant acoustic emission sensors have a clearly defined resonance frequency, but are usually sensitive to other frequencies.

RMS-to-DC ConverterAn electronic device that converts an alternating signal to a voltage level proportional to the average power in the signal.

Signal FilteringFiltering a signal means attenuating frequencies outside a prescribed range. In acoustic emission work, band-pass filtering is used to improve the signal-to-noise ratio by attenuating noise outside the bandwidth of the sensor. Low-pass filtering is used to remove frequencies higher than the Nyquist frequency in order to prevent aliasing.

Transverse ModeA mode of wave propagation where the displacement of the material is perpendicular to the direction of propagation. These modes are only encountered in solid materials.

White NoiseThe characteristic of white noise is a power spectrum of uniform spectral density and is associated with purely random processes.